A reversed-phase liquid chromatography-ultraviolet (LC-UV) method is proposed for the rapid simultaneous analysis of the main carboxylic acids and polyphenols in must and wine. Good resolution was obtained for citric, tartaric, malic, lactic, acetic, caffeic, ellagic and gallic acids, (-)-epicatechin, quercetin and resveratrol. A novel silica-based column containing ether-linked phenyl groups, with polar end-capping and suitable for low-pH aqueous mobile phases was used and found to be superior to others tested. The method employed a mixture of 0.2% TFA in water and acetonitrile as eluents, showed linearity and precision, and was applied to samples of must and wine.